CN115536005B - Carbon nano tube purification method - Google Patents
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- CN115536005B CN115536005B CN202211347132.2A CN202211347132A CN115536005B CN 115536005 B CN115536005 B CN 115536005B CN 202211347132 A CN202211347132 A CN 202211347132A CN 115536005 B CN115536005 B CN 115536005B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 116
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000000746 purification Methods 0.000 title abstract description 19
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 40
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 36
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 230000035484 reaction time Effects 0.000 claims description 18
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000005265 energy consumption Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 230000009471 action Effects 0.000 description 10
- 239000012299 nitrogen atmosphere Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 block Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The invention relates to the technical field of carbon nanotubes, in particular to a carbon nanotube purifying method. The method comprises the following steps: (1) Mixing the carbon nano tube with ammonium chloride solid powder in a first container, and reacting at 350-400 ℃; (2) The carbon nano tube treated in the step (1) is contacted with fluidifying gas, oxygen and carbon dioxide in a second container, and the reaction temperature is 640-690 ℃; (3) And (3) mixing the carbon nano tube treated in the step (2) with fluidizable gas in a third container and cooling. The purification method has no acid washing, water treatment and high energy consumption drying procedures, solves the problems of high energy consumption and serious conductivity damage of the carbon nano tube caused by high-temperature purification, has simple and convenient process and low operation energy consumption, can realize continuous purification of large-batch carbon nano tubes, and can reach the purity of more than 99.9 percent.
Description
Technical Field
The invention relates to the technical field of carbon nanotubes, in particular to a carbon nanotube purifying method.
Background
Since Lijima unexpectedly found multi-wall carbon nanotubes in 1991 in the experimental product of preparing C 60 by vacuum arc evaporation of graphite electrodes, carbon nanotubes as a one-dimensional nanomaterial have been widely developed and applied due to their high mechanical strength, excellent electrical conductivity, and high specific surface area. Carbon nanotubes are mainly coaxial round tubes with single or multiple layers of carbon atoms arranged in a hexagonal manner. It has a very large aspect ratio, typically between 1-100nm in diameter and several microns to hundreds of microns in length. Due to the large length-diameter ratio, the carbon nano tube has excellent mechanical, electrical, electric and heat conductivity. The carbon nano tube has wide potential application prospect in various fields such as lithium ion batteries, coatings, catalyst carriers, rubber plastic composite materials, electrochemical materials, photoelectric sensing and the like.
The preparation method of the carbon nano tube comprises the following steps: graphite arc method, chemical vapor deposition method, laser evaporation graphite method, template method, condensed phase electrolysis method, organic plasma spraying method, etc. Among them, graphite arc process and chemical vapor deposition process are the most widely used preparation processes at present. The carbon nanotubes prepared by these methods are accompanied by a considerable amount of impurities such as carbon nanoparticles, amorphous carbon, catalysts, etc. The presence of these impurities represents a great impediment to the application of carbon nanotubes in a number of fields, and thus research into carbon nanotube purification techniques is urgent. The current industrial batch purification method of the carbon nano tube mainly comprises the following steps: chemical oxidation, gas phase oxidation, liquid phase pickling, high temperature purification, and the like. However, these methods have different problems, and the purity of purification by chemical oxidation and gas phase oxidation is limited; the acid washing method needs to wash with purified water for many times until the pH value is close to neutral, more waste water can be generated, the water resource usage amount is large, and the water is required to be dried again after washing, so that a large amount of electric energy or natural gas energy is consumed, and the energy conservation and emission reduction are not facilitated; the high-temperature purification method for purifying the carbon nano tube requires high temperature of 1800-2500 ℃, has extremely high energy consumption and extremely high damage to the conductivity of the carbon nano tube, so that the invention is highly needed to invent a method for continuously purifying the carbon nano tube in batches with low energy consumption.
Disclosure of Invention
Aiming at the technical problems that the existing carbon nano tube industrialized batch purification method is not ideal in purification effect, large in resource and energy consumption and detrimental to the performance of the carbon nano tube, the invention provides the carbon nano tube purification method which has no acid washing, water treatment and high-energy drying procedures, and avoids the problems of high energy consumption and serious damage to the conductivity of the carbon nano tube caused by high-temperature purification, and has the advantages of simple and convenient process, low operation energy consumption, realization of continuous purification of the carbon nano tube in large batch, and the purity of the carbon nano tube can reach more than 99.9%.
The technical scheme of the invention is as follows:
A method for purifying carbon nanotubes, comprising the steps of:
(1) Mixing the carbon nano tube with ammonium chloride solid powder in a first container, and reacting at 350-400 ℃;
(2) The carbon nano tube treated in the step (1) is contacted with fluidifying gas, oxygen and carbon dioxide in a second container, and the reaction temperature is 640-690 ℃;
(3) And (3) mixing the carbon nano tube treated in the step (2) with fluidizable gas in a third container and cooling.
Furthermore, the purification method is applicable to single-wall carbon nanotubes, double-wall carbon nanotubes or multi-wall carbon nanotubes; the carbon nanotubes may be in the form of powder, granule, block, or a mixture of the three; the preparation method of the carbon nano tube can be a graphite arc method, a chemical vapor deposition method, a laser evaporation graphite method, a template method and an organic plasma spraying method which adopt or not adopt a metal catalyst, and the metal catalyst can be iron, diamond, nickel, magnesium, aluminum, manganese, molybdenum, vanadium and the like.
In the step (1), the reaction is carried out in a fluidifying gas atmosphere, wherein the ammonium chloride accounts for 0.5% -2% of the weight of the carbon nano tube, and the reaction time is 20-40 min.
Further, in the step (1), the carbon nanotubes are preferably placed in a fluidizable gas atmosphere of a first container, and ammonium chloride solid powder is added, wherein the ammonium chloride accounts for 1% of the weight of the carbon nanotubes, the reaction temperature is 370 ℃, and the reaction time is 30min.
Further, after the carbon nanotubes are processed in the step (1), the carbon nanotubes are pushed into the second container by the pushing force of the fluidizing gas stream.
Further, in the step (2), fluidizing gas, oxygen and carbon dioxide are continuously introduced into the second container, the flow rate of the fluidizing gas is 500-600 m 3/h, the flow rate of the oxygen is 200-300 m 3/h, the flow rate of the carbon dioxide is 300-350 m 3/h, and the reaction time is 10-30 min.
Further, the reaction temperature in the step (2) is preferably 670℃and the reaction time is preferably 20 minutes.
Further, after the carbon nanotubes are processed in the step (2), the carbon nanotubes are introduced into the third container by the pushing force of the fluidizing gas stream.
Further, in the step (3), fluidizing gas is continuously introduced into the third container, the flow rate of the fluidizing gas is 300-350 m 3/h, until the temperature of the carbon nanotubes is reduced to room temperature, and the cooling time is about 30min.
Further, the fluidizing gas flow rate in the step (3) is preferably 320m 3/h.
Further, the fluidizing gas is nitrogen or argon.
The invention has the beneficial effects that:
According to the invention, ammonium chloride powder is used as a reaction reagent, and metal impurities of the carbon nano tube are effectively removed at the temperature of 350-400 ℃; nitrogen or argon is used as fluidizing gas, carbon dioxide is used as reducing gas, and oxygen is used as oxidizing gas, so that carbon impurities are effectively removed;
The invention can remove impurities without damaging the carbon tube, avoids using a pickling method and a large amount of water washing purification, effectively reduces the waste of water resources, avoids the subsequent sewage treatment process, and saves the cost; high energy consumption of the high-temperature purification method is avoided. The invention has the advantages of simple process, convenient and quick operation, lower cost and the like, the product purity uniformity is good, the batch stability is good, the invention is suitable for continuous batch purification of carbon nanotubes, and the purity of the obtained carbon nanotubes reaches more than 99.9 percent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a TEM image of a low purity carbon nanotube in the prior art.
FIG. 2 is a TEM image of the high purity carbon nanotubes purified in example 1.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purifying method comprises the following steps of:
(1) And (3) placing the carbon nano tube in a first storage tank of the fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the ammonium chloride accounts for 1% of the weight of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 20min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank of the fluidized bed under the action of pushing force of nitrogen flow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow speed of the nitrogen is 550m 3/h, the flow speed of the oxygen is 250m 3/h, the flow speed of the carbon dioxide is 330m 3/h, the reaction temperature is 680 ℃, and the reaction time is 20min.
(3) And (3) after the carbon nano tube is processed in the step (2), the carbon nano tube enters a third storage tank of the fluidized bed under the action of pushing force of nitrogen flow, and nitrogen is continuously introduced into the third storage tank, so that the carbon nano tube is kept in the nitrogen atmosphere with the flow rate of 330m 3/h until the temperature of the carbon nano tube is reduced to room temperature, and the cooling time is about 30min, so that the carbon nano tube with the purity of over 99.9 percent is obtained.
Example 2
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purifying method comprises the following steps of:
(1) And (3) placing the carbon nano tube in a first storage tank of the fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the ammonium chloride accounts for 1% of the weight of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 20min.
(2) After the carbon nano tube is processed in the step (1), the carbon nano tube enters a second storage tank under the action of the pushing force of argon gas flow, argon gas, oxygen and carbon dioxide are continuously introduced into the second storage tank, the flow rate of the argon gas is 500m 3/h, the flow rate of the oxygen gas is 250m 3/h, the flow rate of the carbon dioxide is 330m 3/h, the reaction temperature is 680 ℃, and the reaction time is 20min.
(3) And (3) after the carbon nano tube is processed in the step (2), enabling the carbon nano tube to enter a third storage tank under the action of pushing force of argon gas flow, continuously introducing argon gas into the third storage tank, and keeping the carbon nano tube in the argon gas atmosphere with the flow rate of 330m 3/h until the temperature of the carbon nano tube is reduced to room temperature, and cooling for about 30min, thus obtaining the carbon nano tube with the purity of over 99.9 percent.
Example 3
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purifying method comprises the following steps of:
(1) And (3) placing the carbon nano tube in a first storage tank of the fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the ammonium chloride accounts for 0.5% of the weight of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 20min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank under the action of pushing force of nitrogen flow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow speed of the nitrogen is 550m 3/h, the flow speed of the oxygen is 250m 3/h, the flow speed of the carbon dioxide is 330m 3/h, the reaction temperature is 690 ℃, and the reaction time is 20min.
(3) And (3) after the carbon nano tube is processed in the step (2), enabling the carbon nano tube to enter a third storage tank under the action of pushing force of nitrogen flow, continuously introducing nitrogen into the third storage tank, and keeping the carbon nano tube in a nitrogen atmosphere with the flow rate of 320m 3/h until the temperature of the carbon nano tube is reduced to room temperature, and cooling for about 30min, thus obtaining the carbon nano tube with the purity of over 99.9 percent.
Example 4
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purifying method comprises the following steps of:
(1) And (3) placing the carbon nano tube in a first storage tank of the fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the ammonium chloride accounts for 2% of the weight of the carbon nano tube, the reaction temperature is 350 ℃, and the reaction time is 40min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank under the action of pushing force of nitrogen flow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow speed of the nitrogen is 600m 3/h, the flow speed of the oxygen is 200m 3/h, the flow speed of the carbon dioxide is 350m 3/h, the reaction temperature is 645 ℃, and the reaction time is 30min.
(3) And (3) after the carbon nano tube is processed in the step (2), enabling the carbon nano tube to enter a third storage tank under the action of pushing force of nitrogen flow, continuously introducing nitrogen into the third storage tank, and keeping the carbon nano tube in a nitrogen atmosphere with the flow rate of 300m 3/h until the temperature of the carbon nano tube is reduced to room temperature, and cooling for about 30min, thus obtaining the carbon nano tube with the purity of over 99.9 percent.
Example 5
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purifying method comprises the following steps of:
(1) And (3) placing the carbon nano tube in a first storage tank of the fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the ammonium chloride accounts for 1% of the weight of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 30min.
(2) After the carbon nano tube is processed in the step (1), the carbon nano tube enters a second storage tank under the action of pushing force of nitrogen flow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow rate of the nitrogen is 530m 3/h, the flow rate of the oxygen is 270m 3/h, the flow rate of the carbon dioxide is 340m 3/h, the reaction temperature is 670 ℃, and the reaction time is 20min.
(3) And (3) after the carbon nano tube is processed in the step (2), enabling the carbon nano tube to enter a third storage tank under the action of pushing force of nitrogen flow, continuously introducing nitrogen into the third storage tank, and keeping the carbon nano tube in a nitrogen atmosphere with the flow rate of 320m 3/h until the temperature of the carbon nano tube is reduced to room temperature, and cooling for about 30min, thus obtaining the carbon nano tube with the purity of over 99.9 percent.
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims.
Claims (10)
1. A method for purifying a carbon nanotube, comprising the steps of:
(1) Mixing carbon nano tubes with ammonium chloride solid powder in a first container, wherein the ammonium chloride accounts for 0.5-2% of the weight of the carbon nano tubes, and reacting at 350-400 ℃;
(2) The carbon nano tube treated in the step (1) is contacted with fluidifying gas, oxygen and carbon dioxide in a second container, and the reaction temperature is 640-690 ℃;
the reaction time is 10-30min;
(3) And (3) mixing the carbon nano tube treated in the step (2) with fluidizable gas in a third container and cooling.
2. The method of purifying a carbon nanotube as claimed in claim 1, wherein in the step (1), the reaction is performed under a fluidizable gas atmosphere for a reaction time of 20 to 40 minutes.
3. The method of purifying carbon nanotubes of claim 1, wherein step (1) is specifically to place the carbon nanotubes in a first container in a fluidizable gas atmosphere, adding ammonium chloride solid powder, wherein the ammonium chloride is 1% by weight of the carbon nanotubes, and the reaction temperature is 370 ℃ and the reaction time is 30min.
4. The method of claim 1, wherein the carbon nanotubes are introduced into the second vessel by pushing force of the fluidizing gas stream after the carbon nanotubes are treated in step (1).
5. The method of purifying carbon nanotubes according to claim 1, wherein in the step (2), fluidizing gas, oxygen and carbon dioxide are continuously introduced into the second vessel, the flow rate of the fluidizing gas is 500 to 600m 3/h, the flow rate of the oxygen is 200 to 300m 3/h, and the flow rate of the carbon dioxide is 300 to 350m 3/h.
6. The method of purifying carbon nanotubes of claim 1, wherein the reaction temperature in step (2) is 670 ℃ and the reaction time is 20min.
7. The method of claim 1, wherein the carbon nanotubes are introduced into the third vessel by pushing force of the fluidizing gas stream after the carbon nanotubes are treated in step (2).
8. The method of purifying carbon nanotubes according to claim 1, wherein in the step (3), the fluidizing gas is continuously introduced into the third vessel at a flow rate of 300 to 350m 3/h until the temperature of the carbon nanotubes is lowered to room temperature.
9. The method of purifying a carbon nanotube according to claim 8, wherein the fluidizing gas in the step (3) has a flow rate of 320m 3/h.
10. The method of claim 1, wherein the fluidizing gas is nitrogen or argon.
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| CN202211347132.2A CN115536005B (en) | 2022-10-31 | Carbon nano tube purification method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211347132.2A CN115536005B (en) | 2022-10-31 | Carbon nano tube purification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041427A (en) * | 2006-03-22 | 2007-09-26 | 索尼株式会社 | Manufacturing method of carbon material, carbon material and manufacturing method of electronic components |
| CN101941691A (en) * | 2010-09-21 | 2011-01-12 | 上海大学 | Preparation method of single-walled carbon nanotube |
| CN106315560A (en) * | 2016-08-22 | 2017-01-11 | 赖世权 | Carbon nanotube purification method |
| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
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| Title |
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| Purification of double-walled carbon nanotube macro-films;Yun Chen等;《NewJ.Chem》;第542–545页 * |
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